CN102545053B - Visible electric pumping random laser device with adjustable wavelength and preparation method thereof - Google Patents
Visible electric pumping random laser device with adjustable wavelength and preparation method thereof Download PDFInfo
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- CN102545053B CN102545053B CN 201110456104 CN201110456104A CN102545053B CN 102545053 B CN102545053 B CN 102545053B CN 201110456104 CN201110456104 CN 201110456104 CN 201110456104 A CN201110456104 A CN 201110456104A CN 102545053 B CN102545053 B CN 102545053B
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Abstract
The invention discloses a visible electric pumping random maser device adjustable wavelength and a preparation method thereof. The preparation method of the device comprises the following steps of: depositing a CdZno film on a substrate by adopting a sputtering method, and carrying out rapid thermal treatment under inert gas atmosphere; depositing an SiO2 film on the CdZnO film by adopting a sol-gel method; depositing a semitransparent Au electrode on the SiOe film by adopting the sputtering method, and depositing an ohmic contact electrode on the back of the substrate. According to the invention, the CdZnO film is adopted as a main material, and rapid thermal treatment is carried out on the CdZno film after the deposition of the CdZnO film, and finally the electric pumping random maser device with the Au/SiO2/CdZno MIS structure is prepared. Under certain forward bias, the device can send out electric pumping random maser waves positioned in a visible area; and according to differentrapid thermal treatment temperatures, the center wavelength of the random mastering bands is within the range of 485nm-430nm and is adjustable. The device has a simple structure and is easy to realize; and facilities adopted in the preparation process are compatible with the existing mature process of silicon devices.
Description
Technical field
The present invention relates to a kind of electric pumping random Amplifier Based On Stimulated Emission Of Radiation spare, be specially a kind of based on Au/SiO on the silicon substrate
2Visible electric pumping random Amplifier Based On Stimulated Emission Of Radiation spare and the preparation method of the wavelength-tunable of/CdZnO MIS structure.
Background technology
Because the development of photoelectric technology to the demand of ultraviolet, visual field Laser Devices and other short-wavelength light electric devices, makes the Random Laser research of ZnO receive increasing concern.As the important a member in the ZnO system, the CdZnO film is by regulating the content of Cd, can be effectively the emission wavelength of CdZnO film be adjusted to visible region.(J.A.Van?Vechten?and?T.K.Bergstresser，Phys.Rev.B.1，3351(1970))。Penetrate luminously if can utilize the CdZnO film to be implemented in swashing at random of visual field, to have active operation significance undoubtedly.
The research of penetrating that swashs at random for the CdZnO film at present mainly concentrates on optical pumping sharp penetrating at random, for the sharp report of penetrating of electric pumping random also seldom.Its main bottleneck is that the one side solid solubility of CdO in the CdO-ZnO alloy system very low (approximately having only 2mol% under thermal equilibrium state) is so be difficult to utilize simple equipment to prepare the CdZnO film of high Cd content.The molten boiling point that Cd is lower makes that again preparation becomes very difficult based on the CdZnO membrane electro luminescent device of high Cd doped in concentrations profiled on the other hand.
Horse waited the people to utilize metal-insulator layer-semiconductor (MIS) structure on the sunny side in 2007, successfully realized sharp (the Xiangyang Ma that penetrates of electric pumping random of ZnO film, Peiliang Chen, DongshengLi, Yuanyuan Zhang, and Deren Yang, Appl.Phys.Lett.90,231106 (2007)).Publication number is that the application for a patent for invention of CN102290707A discloses a kind of ultraviolet and electric pumping random Amplifier Based On Stimulated Emission Of Radiation spare and preparation method visible and that deposit, the SiO that utilized CdO-ZnO counterdiffusion film preparation
2/ ZnO-CdO/SiO
2The dual potential barrier structure device can send the electric pumping random that is positioned at ultraviolet, visual field and swash and to penetrate.On this research basis, how to realize that the CdZnO film sends sharp the penetrating of electric pumping random of wavelength-tunable in the visual field, be a difficult problem needing solution badly.
Summary of the invention
The invention provides a kind of preparation method of electric pumping random Amplifier Based On Stimulated Emission Of Radiation spare, technology is simple, with the silicon device process compatible of existing maturation.By the electric pumping random Amplifier Based On Stimulated Emission Of Radiation spare that this method makes, can realize the CdZnO film the electric pumping random of the wavelength-tunable of visual field swash penetrate luminous.
A kind of preparation method of electric pumping random Amplifier Based On Stimulated Emission Of Radiation spare comprises:
(1) adopts sputtering method at substrate deposition CdZnO film, under inert gas atmosphere, carry out rapid thermal treatment again;
(2) adopt sol-gel process to deposit SiO at the CdZnO film
2Film;
(3) adopt sputtering method at SiO
2The translucent Au electrode of deposition on the film is at substrate back deposition Ohm contact electrode.
In the step (1), described substrate can be the N-type silicon chip of 0.005～50 ohmcm for resistivity.
Described substrate temperature is preferably 400～700 ℃; More preferably 600 ℃.Cross low underlayer temperature enough activation energies can not be provided for the doping of Cd atom, and too high underlayer temperature can cause Cd volatilization again from the film that has prepared.
Preferably, the used target of deposition CdZnO film is the CdZnO ceramic target, and the Cd doping counts 20% with molar content in the CdZnO ceramic target.The CdZnO ceramic target can adopt the commercial goods.
Described inert gas can be argon gas or nitrogen.
Preferably, the temperature of described rapid thermal treatment (RTP) is 800～900 ℃, and the quick heat treatment time is 1～200 second.CdZnO film defects without high-temperature process is more, luminous a little less than; The conventional heating process processing time is longer, causes the phase-splitting of CdZnO or the volatilization of Cd easily.And adopt rapid thermal treatment condition provided by the invention, help to reduce the phase-splitting of CdZnO film, and can make the luminous enhancing of nearly band edge.
Adopt different temperatures that the CdZnO film is carried out rapid thermal treatment, can prepare the different electric pumping random Amplifier Based On Stimulated Emission Of Radiation spare of nearly band edge emission wavelength, realize the adjustable of wavelength.
In the step (2), preferably, deposition SiO
2Carry out heat treated behind the film, the heat treated temperature is 300～400 ℃, and the heat treated time is 1～2 hour.By heat treated, can remove the organic substance in the film, help film forming.
The present invention also provides a kind of electric pumping random Amplifier Based On Stimulated Emission Of Radiation spare that adopts above-mentioned preparation method to make, and the substrate face of this device deposits CdZnO film, SiO from bottom to top successively
2Film and Au electrode, substrate back deposits Ohm contact electrode.Result of the test shows, this device can send the electric pumping random that is positioned at the visual field and swash and penetrate, and it is adjustable to swash the centre wavelength of penetrating band at random.
The present invention swashs the main material of penetrating with the CdZnO film as electric pumping random, behind deposition CdZnO film it is carried out rapid thermal treatment simultaneously, has prepared Au/SiO
2The electric pumping random Amplifier Based On Stimulated Emission Of Radiation spare of/CdZnO MIS structure.Because the CdZnO film has been carried out the rapid thermal treatment under the inert gas atmosphere, tangible phase-splitting does not take place in CdZnO thin-film light emitting layer substantially, make CdZnO film (substrate connects negative voltage) under certain forward bias, can send the electric pumping random that is positioned at the visual field and swash and to penetrate; And, along with the rising of rapid heat-treatment temperature, the nearly band edge emission wavelength blue shift gradually that Cd can volatilize gradually and cause the CdZnO film, according to different rapid heat-treatment temperatures, it swashs the centre wavelength of penetrating band at random and can regulate in 485nm～430nm scope.
Structure and the implementation of device of the present invention are simple, preparation technology and used equipment and the silicon device process compatible of existing maturation.
Description of drawings
Fig. 1 is the structural representation of device of the present invention;
Fig. 2 be the CdZnO film respectively through after following 800 ℃, 850 ℃, 900 ℃ RTP heat treatments of argon gas and the XRD collection of illustrative plates of ZnO film after the following 800 ℃ of RTP heat treatments of argon gas;
Fig. 3 be the CdZnO film respectively through after following 800 ℃, 850 ℃, 900 ℃ RTP heat treatments of argon gas and the room temperature PL spectrum of ZnO film after the following 800 ℃ of RTP heat treatments of argon gas;
Fig. 4 (a) is the room temperature EL spectrum of the embodiment of the invention 1 device under different forward biases, i.e. Au/SiO
2The room temperature EL spectrum of/CdZnO MIS structure devices under different forward biases, wherein the CdZnO film is through the following 800 ℃ of RTP heat treatments of argon gas; Fig. 4 (b) is that the observable Output optical power of the embodiment of the invention 1 device is with the change curve of injection electric current;
Fig. 5 is the room temperature EL spectrum of embodiment of the invention 1-3 and Comparative Examples 1 device, i.e. Au/SiO
2/ CdZnO MIS structure devices and Au/SiO
2The room temperature EL spectrum of/ZnO MIS structure devices, wherein the CdZnO film is respectively through following 800 ℃, 850 ℃, 900 ℃ RTP heat treatments of argon gas, and ZnO film is through the following 800 ℃ of RTP heat treatments of argon gas.
Embodiment
As Fig. 1, a kind of electric pumping random Amplifier Based On Stimulated Emission Of Radiation spare comprises substrate 1, and substrate 1 front deposits CdZnO film 2, SiO from bottom to top successively
2Film 3 and translucent Au electrode 4, substrate 1 backside deposition has Ohm contact electrode 5.Substrate is selected silicon chip for use, and resistivity is generally 0.005～50 ohmcm.Embodiment 1-3 has prepared the device of said structure, and is specific as follows:
Embodiment 1-3
1) clean N-type＜100 〉, resistivity is that 0.005 ohmcm, size are 15 * 15mm
2, thickness is 675 microns silicon chip;
2) utilize radio frequency sputtering at Si substrate deposition CdZnO film, target is the CdZnO ceramic target of Cd doping content 20atom%, and underlayer temperature is 600 ℃, and sputtering power is 100W, Ar, O
2Flow be respectively 30: 15, air pressure is 3.5Pa, sputtering time 1 hour, the about 120nm of film thickness.The deposition back is passed through RTP heat treatment respectively under Ar atmosphere, the processing time is 1 minute;
Wherein, the RTP heat treatment temperature of embodiment 1-3 is respectively 800 ℃, 850 ℃ and 900 ℃;
3) utilize tetraethoxysilane, alcohol, watery hydrochloric acid prepare SiO by a certain percentage
2Colloidal sol; Spin coating one deck SiO on silicon chip
2Film was dried 10 minutes for 100 ℃, at O
2The following 400 ℃ of heat treatments of atmosphere 1 hour;
4) at SiO
2The thick translucent Au electrode of the about 20nm of sputter on the film, and the Au electrode that the about 100nm of sputter is thick on the silicon substrate back side (Ohm contact electrode 5); Sputtering power is 45W, and the Ar flow is 20, and air pressure 10Pa, underlayer temperature are 150 ℃; Front electrode sputter 30 seconds, backplate sputter 3 minutes.
Comparative Examples 1 substitutes the CdZnO film according to above-mentioned steps with ZnO film, through the following 800 ℃ of RTP heat treatments of Ar atmosphere, and preparation Au/SiO
2The electric pumping random Amplifier Based On Stimulated Emission Of Radiation spare of/ZnO MIS structure.
Fig. 2 be the CdZnO film respectively through after following 800 ℃, 850 ℃, 900 ℃ RTP heat treatments of argon gas and the XRD collection of illustrative plates of ZnO film after the following 800 ℃ of RTP heat treatments of argon gas.As we can see from the figure, all there is main relevant (103) diffraction maximum of hexagonal buergerite in various CdZnO films.With finding that (103) diffraction maximum of various CdZnO films is compared all with pure ZnO film and produced tangible movement to the low-angle direction after the ZnO film contrast, this is because the doping of Cd causes CdZnO film lattice constant to become big cause.Along with the rising of RTP heat treatment temperature, (103) diffraction maximum of CdZnO film reduces gradually to the movement of little angle of diffraction direction, and the rising of this explanation RTP heat treatment temperature can make the doping of Cd in the CdZnO film reduce.Except (103) diffraction maximum, also have some faint cube to reach the relevant diffraction maximum of hexagonal buergerite mutually and exist in the CdZnO film, the CdZnO film of this explanation after different temperatures RTP heat treatment produced slight phase-splitting.
Fig. 3 provided the CdZnO film respectively through after following 800 ℃, 850 ℃, 900 ℃ RTP heat treatments of argon gas and the room temperature PL spectrum of ZnO film after the following 800 ℃ of RTP heat treatments of argon gas.As can be seen from the figure, various CdZnO films have all produced single nearly band edge radioluminescence peak at visible region.PL spectrum with ZnO film is compared and can be found, tangible red shift has all taken place the PL glow peak of various CdZnO films, and this explanation has formed the CdZnO film that different Cd components are mixed.Along with the rising of RTP heat treatment temperature, the peak position at the radioluminescence peak of film is blue shift gradually, wavelength at 490nm to regulating between the 425nm.
Fig. 4 (a) is the room temperature EL spectrum of device under different forward biases of embodiment 1, i.e. Au/SiO
2The room temperature EL spectrum of/CdZnO MIS structure devices under different forward biases, wherein the CdZnO film is through the following 800 ℃ of RTP heat treatments of argon gas, this moment SiO
2Au electrode on the film just connects, and the Au electrode of Si substrate back connects negative.As we can see from the figure, sharp-pointed glow peak has all appearred in device in the visible region, and the centre wavelength of its glow peak band is about 480nm.Along with the increase of injecting electric current, the intensity of glow peak also obviously increases thereupon.And the spacing of glow peak does not wait, and its spectral line pattern also changes along with the difference that applies bias voltage.Above phenomenon illustrates that this device has produced sharp penetrating at random in the visual field.Fig. 4 (b) is that the observable Output optical power of this device is with the change curve of injection electric current.Can see that there is tangible threshold current in device, above behind its threshold current, the detectable Output optical power of device increases rapidly along with the increase of injecting electric current.
Fig. 5 is the room temperature EL spectrum of embodiment 1-3 and Comparative Examples 1 device, i.e. Au/SiO
2/ CdZnOMIS structure devices and Au/SiO
2The room temperature EL spectrum of/ZnO MIS structure devices, wherein the CdZnO film is respectively through following 800 ℃, 850 ℃, 900 ℃ RTP heat treatments of argon gas, and ZnO film is through the following 800 ℃ of RTP heat treatments of argon gas.Can see various Au/SiO
2/ CdZnO MIS structure devices has all produced in the visual field to swash at random and has penetrated; With Au/SiO
2The EL spectrum of/ZnO MIS structure devices compares and can find, it swashs the centre wavelength of penetrating at random all tangible red shift.And along with the rising of CdZnO film RTP heat treatment temperature, swash the centre wavelength blue shift gradually penetrate band at random, at 485nm to regulating between the 430nm.
Claims (7)
1. the preparation method of an electric pumping random Amplifier Based On Stimulated Emission Of Radiation spare comprises:
(1) adopts sputtering method at substrate deposition CdZnO film, under inert gas atmosphere, carry out rapid thermal treatment again;
(2) adopt sol-gel process to deposit SiO at the CdZnO film
2Film;
(3) adopt sputtering method at SiO
2The translucent Au electrode of deposition on the film is at substrate back deposition Ohm contact electrode;
In the step (1), described quick heat treatment temperature is 800～900 ℃, and the quick heat treatment time is 1～200 second.
2. preparation method according to claim 1 is characterized in that, in the step (1), described substrate is that resistivity is the N-type silicon chip of 0.005～50 ohmcm.
3. preparation method according to claim 1 is characterized in that, in the step (1), described substrate temperature is 400～700 ℃.
4. preparation method according to claim 1 is characterized in that, in the step (1), the used target of deposition CdZnO film is the CdZnO ceramic target, and the Cd doping counts 20% with molar content in the CdZnO ceramic target.
5. preparation method according to claim 1 is characterized in that, in the step (1), described inert gas is argon gas or nitrogen.
6. preparation method according to claim 1 is characterized in that, in the step (2), and deposition SiO
2Carry out heat treated behind the film, the heat treated temperature is 300～400 ℃, and the heat treated time is 1～2 hour.
7. the electric pumping random Amplifier Based On Stimulated Emission Of Radiation spare that makes of an employing such as the arbitrary described preparation method of claim 1-6.
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| CN102545053B true CN102545053B (en) | 2013-10-09 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102290707A (en) * | 2011-07-12 | 2011-12-21 | 浙江大学 | Ultraviolet-visible coexisting electrically pumped random laser device and preparation method thereof |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102290707A (en) * | 2011-07-12 | 2011-12-21 | 浙江大学 | Ultraviolet-visible coexisting electrically pumped random laser device and preparation method thereof |
Non-Patent Citations (6)
| Title |
|---|
| Effect of rapid thermal annealing on photoluminescence and crystal structures of CdZnO films;Ruijie Zhang et al.;《Journal of Crystal Growth》;20100316;第312卷;第1908页第2部分-实验流程 * |
| Electrically pumped wavelength-tunable ultraviolet random lasing from MgxZn1-xO films on Si;Ye Tian et al.;《Optics Express》;20100506;第18卷(第10期);第10669页第2部分-实验明细 * |
| Optical properties of sputtered hexagonal CdZnO films with band gap energies from 1.8 to 3.3 eV;Xiangyang Ma et al.;《Journal of Alloys and Compounds》;20110329;第509卷;6599-6602 * |
| Ruijie Zhang et al..Effect of rapid thermal annealing on photoluminescence and crystal structures of CdZnO films.《Journal of Crystal Growth》.2010,第312卷 |
| Xiangyang Ma et al..Optical properties of sputtered hexagonal CdZnO films with band gap energies from 1.8 to 3.3 eV.《Journal of Alloys and Compounds》.2011,第509卷 |
| Ye Tian et al..Electrically pumped wavelength-tunable ultraviolet random lasing from MgxZn1-xO films on Si.《Optics Express》.2010,第18卷(第10期), |
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